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使用区域选择性阿佩尔反应从d-果糖和l-山梨糖多克级合成2,5-二脱氧-2,5-亚氨基-d-甘露糖醇(DMDP)和2,5-二脱氧-2,5-亚氨基-d-葡萄糖醇(DGDP)。

Multigram-Scale Synthesis of 2,5-Dideoxy-2,5-imino-d-mannitol (DMDP) and 2,5-Dideoxy-2,5-imino-d-glucitol (DGDP) from d-Fructose and l-Sorbose Using a Regioselective Appel Reaction.

作者信息

Sunde-Brown Peter, Miller Gavin J, Houston Todd A

机构信息

Institute for Glycomics, Griffith University, Gold Coast Campus, Southport 4215 , Queensland, Australia.

School of Chemical and Physical Sciences and Centre for Glycoscience, Keele University, Keele, Staffordshire ST5 5BG, U.K.

出版信息

J Org Chem. 2025 Feb 14;90(6):2288-2297. doi: 10.1021/acs.joc.4c02667. Epub 2025 Feb 5.

Abstract

We report a practical 5 g scale stereoselective synthesis of the valuable iminosugar DMDP from d-fructose in only 7 synthetic steps and in a 70% overall yield, which doubles previously reported yields. This process requires only two chromatographic purification steps, taking advantage of a regioselective Appel reaction. The regioselective reaction has also been applied on a similar scale to prepare the C-2 diastereomer of DMDP, DGDP, from l-sorbose in 7 steps (two purifications) and 56% overall yield, albeit with diminished diastereomeric purity (d.r. 90:10). The C-5 regioselectivity has also been illustrated on d-psicose and d-tagatose, making this an attractive method for preparing pyrrolidine iminosugars or 5-thiosugars from ketopyranoses.

摘要

我们报道了一种实用的5克规模的立体选择性合成方法,以d-果糖为原料,仅通过7步合成即可得到有价值的亚氨基糖DMDP,总产率为70%,是此前报道产率的两倍。该过程仅需两步柱色谱纯化,利用了区域选择性Appel反应。该区域选择性反应也已应用于类似规模的反应,以l-山梨糖为原料,通过7步反应(两步纯化)制备DMDP的C-2非对映异构体DGDP,总产率为56%,尽管非对映体纯度有所降低(d.r. 90:10)。C-5区域选择性也已在d-阿洛酮糖和d-塔格糖上得到证实,这使得该方法成为从酮吡喃糖制备吡咯烷亚氨基糖或5-硫代糖的一种有吸引力的方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9976/11833879/75c50d70e7d5/jo4c02667_0001.jpg

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